A new cermet-based composite material and its preparation method

The novel metal ceramic composite material with TiC and stainless steel reinforcement, fabricated via in-situ processing, addresses interface bonding issues, enhancing mechanical and tribological properties for broader industrial applications.

CN117026053BActive Publication Date: 2025-07-15YANSHAN UNIV
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Patent Information

Application Number
CN202310891147.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-07-19
Publication Date
2025-07-15
Estimated Expiration
2043-07-19

AI Technical Summary

Technical Problem

The existing metal cermet matrix composite materials have insufficient interfacial bonding and performance matching, resulting in reduced material strength or insufficient toughness, which makes it difficult to meet the needs of the fields of aerospace, medical care and automobile.

Method used

The in-situ preparation process is adopted, using the TiC ceramic phase as the matrix and combining the 304L stainless steel phase as the reinforced phase. A new metal cermet matrix composite material is prepared through ball milling, discharge plasma sintering and surface treatment to improve its interface bonding, mechanical and friction properties.

Benefits of technology

The prepared new metal cermet matrix composite material has excellent performance in mechanical properties and friction properties, widening its application range, and is suitable for aerospace parts, automotive engines, self-lubricating bearings and high-speed train brake pads.

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Abstract

The present invention provides a novel metal-ceramic matrix composite material and a preparation method thereof, relating to the technical field of metal-ceramic materials. The composite material is composed of the following materials in proportion by weight: titanium powder 35.74 - 67.12 wt.%, silicon powder 6.97 - 12.88 wt.%, graphite powder 0 - 10 wt.%, carbon fiber 0 - 10.72 wt.%, aluminum powder 0 - 2.54 wt.%, and 304L stainless steel powder 5 - 50 wt.%. In order to prepare a novel metal-ceramic matrix composite material with better comprehensive properties, the present invention not only adopts an in-situ preparation process to improve the interfacial bonding between the metal and the ceramic phase, but also uses the TiC ceramic phase as the matrix and the stainless steel phase as the reinforcing phase to comprehensively improve the mechanical and friction properties. The novel metal-ceramic matrix composite material prepared by the present invention has good mechanical and friction properties, and is not only applicable to aerospace parts and automotive engines of traditional metal-ceramic matrix composite materials, but also can be applied to friction fields such as self-lubricating bearings and high-speed train brake pads, broadening the application scope of metal-ceramic matrix composite materials.
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Description

Technical Field

[0001] The present invention relates to the technical field of cermet materials, and in particular, to a novel cermet matrix composite material and a preparation method thereof. Background Art

[0002] Cermet is a multiphase composite material obtained by powder metallurgy process to combine ceramic phase and binder phase. Due to its high hardness, high thermal conductivity, high electrical conductivity, corrosion resistance, fire resistance, radiation resistance, and excellent high-temperature mechanical properties, it can provide better materials for industrial needs and promote the development of fields such as aerospace, medical, automotive, and train.

[0003] However, due to the interfacial bonding between metal and ceramic severely restricting the performance of cermet matrix composites, the stronger the wetting force, the greater the possibility of the metal forming a continuous phase, and the smaller the tendency of ceramic particles to aggregate into large particles, the better the performance of the cermet. Moreover, the linear expansion coefficients and elastic moduli of the metal and ceramic phases should be matched. The smaller the expansion coefficient, the better the thermal shock resistance. However, if the linear expansion coefficient and elastic modulus of the cermet are mismatched, it is easy to cause cracks in the ceramic matrix, reducing the strength of the material, or the cracks avoiding the toughening particles and only expanding in the matrix.

[0004] To make up for the defects of cermet matrix composites, researchers have adopted two approaches to solve them. One is to prepare a Ti(C,N) solid solution phase as the matrix, and the other is to use metal as the matrix to prepare cermet matrix composites. However, these two solutions are to sacrifice some advantageous properties of cermet matrix composites to make up for the deficiencies of other properties. For example, cermet matrix composites with a Ti(C,N) solid solution phase as the matrix have high hardness and high-temperature mechanical properties, but poor toughness; cermet matrix composites with metal as the matrix have good toughness and flexural strength, but low hardness. Summary of the Invention

[0005] In view of this, the purpose of the present invention is to propose a novel cermet matrix composite material and a preparation method thereof. To prepare a novel cermet matrix composite material with better comprehensive performance, the present invention not only adopts an in-situ preparation process to improve the interfacial bonding between metal and ceramic phases, but also uses a TiC ceramic phase as the matrix and a stainless steel phase as the reinforcement phase to comprehensively improve the mechanical and friction properties. The novel cermet matrix composite material prepared by the present invention has good mechanical and friction properties, and is not only applicable to fields such as aerospace parts and automotive engines of traditional cermet matrix composites, but also can be applied to friction fields such as self-lubricating bearings and high-speed train brake pads, expanding the application range of cermet matrix composites.

[0006] The technical means adopted by the present invention are as follows:

[0007] A new cermet-based composite material, and the composite material is composed of the following materials in the following weight ratios: titanium powder 35.74 - 67.12 wt.%, silicon powder 6.97 - 12.88 wt.%, graphite powder 0 - 10 wt.%, carbon fiber 0 - 10.72 wt.%, aluminum powder 0 - 2.54 wt.%, 304L stainless steel powder 5 - 50 wt.%.

[0008] Further, the titanium powder, silicon powder, graphite powder, aluminum powder and 304L stainless steel powder are elemental powders; the purity of the titanium powder, silicon powder, graphite powder, aluminum powder and 304L stainless steel powder is 99%; the particle diameters of the titanium powder, silicon powder, graphite powder, aluminum powder and 304L stainless steel powder are less than 45 μm; the length of the carbon fiber is 3 mm and the diameter is 7 nm.

[0009] A preparation method of a new cermet-based composite material for preparing any of the above new cermet-based composite materials, comprising the following steps:

[0010] S1. Ball-mill several of the titanium powder, silicon powder, graphite powder, carbon fiber, aluminum powder and 304L stainless steel powder in a ball mill, and the mass ratio of balls to materials ranges from 2:1 to 10:1. After ball-milling, separate the raw material powder from the grinding balls in a glove box to obtain the new cermet-based composite material powder;

[0011] S2. Fill the new cermet-based composite material powder obtained in S1 into a cemented carbide mold, pre-press and form it under a pressure of 50 - 300 MPa, then load it into a graphite mold for spark plasma sintering. The sintering pressure is 20 - 50 MPa, the sintering temperature is 1200 - 1600 °C, and it is heated from room temperature to the target sintering temperature at a rate of 50 - 90 °C / min. After reaching the target sintering temperature, keep it warm for 1 - 60 min to obtain the sintered body of the new cermet-based composite material;

[0012] S3. Grind and polish the surface of the sintered body obtained in S2 to remove the residual graphite on the surface of the sintered body and the burrs generated at the edges during the sintering process, thereby obtaining the new cermet-based composite material.

[0013] Further, in S1, the grinding balls are made of three different sizes of cemented carbide balls, the diameter of the large-size cemented carbide ball is 6 mm, the diameter of the medium-size cemented carbide ball is 4 mm, the diameter of the small-size cemented carbide ball is 1 mm, and the mass ratio of the three different sizes of cemented carbide balls is 1:3:6.

[0014] Further, in S1, the set rotation speed range is 200 - 400 r / min, running forward and backward alternately, stopping for 20 - 30 min every 1 h, and the cumulative ball-milling time range is 3 - 10 h.

[0015] Compared with the prior art, the present invention has the following advantages:

[0016] In the novel metal-ceramic matrix composite material of the present invention, an in-situ preparation process is adopted to enhance the interfacial strength between the metal and the ceramic phase.

[0017] In the novel metal-ceramic matrix composite material of the present invention, TiC is used as the matrix and stainless steel is used as the reinforcing phase to improve the mechanical and friction properties of the composite material.

[0018] The novel metal-ceramic matrix composite material of the present invention has good mechanical properties (hardness and toughness) and friction properties (friction coefficient and wear rate at room temperature and 500 °C), which broadens the application range of metal-ceramic matrix composite materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0020] Figure 1 XRD pattern of the novel metal-ceramic matrix composite material prepared in Example 1 of the present invention.

[0021] Figure 2 FESEM images of the fracture surface of the novel metal-ceramic matrix composite material prepared in Example 1 of the present invention: Figure 2 a is the fracture surface morphology of the novel metal-ceramic matrix composite material, Figure 2 b is Figure 2 the enlarged view of the boxed area in a, Figure 2 c is Figure 2 the enlarged view of the boxed area in b, Figure 2 d is Figure 2 the enlarged view of the boxed area in c;

[0022] Figure 3 FESEM images of the room-temperature friction surface of the novel metal-ceramic matrix composite material prepared in Example 1 of the present invention: Figure 3 a is the room-temperature friction surface morphology of the novel metal-ceramic matrix composite material, Figure 3 b is Figure 3 the enlarged view of the boxed area in a, Figure 3 c is Figure 3 the enlarged view of the boxed area in b, Figure 3 d is Figure 3 the enlarged view of the boxed area in c;

[0023] Figure 4 XRD pattern of the novel metal-ceramic matrix composite material prepared in Example 7 of the present invention.

[0024] Figure 5 FESEM image of the polished surface of the novel metal-ceramic matrix composite prepared in Example 7 of the present invention: Figure 5 a is the morphology image of the polished surface of the novel metal-ceramic matrix composite, Figure 5 b is Figure 5 the enlarged image of the area within the square frame of a, Figure 5 c is Figure 5 the enlarged image of the area within the square frame of b, Figure 5 d is Figure 5 the enlarged image of the area within the circle of a;

[0025] Figure 6 FESEM image of the room-temperature friction surface of the novel metal-ceramic matrix composite prepared in Example 7 of the present invention: Figure 6 a is the morphology image of the room-temperature friction surface of the novel metal-ceramic matrix composite, Figure 6 b is Figure 6 the enlarged image of the area within the square frame of a, Figure 6 c is Figure 6 the enlarged image of the area within the circle of a, Figure 6 d is Figure 6 the enlarged image of the area within the square frame of c. Detailed implementation manners

[0026] It should be noted that, without conflict, the embodiments in the present invention and the features in the embodiments can be combined with each other. The described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. The following description of at least one exemplary embodiment is actually only illustrative and in no way constitutes a limitation to the present invention and its application or use. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0027] The present invention provides a novel metal-ceramic matrix composite and its preparation method. The mass percentage of the chemical components of the novel metal-ceramic matrix composite is 35.74 - 67.12 wt.% of titanium powder, 6.97 - 12.88 wt.% of silicon powder, 0 - 10 wt.% of graphite powder, 0 - 10.72 wt.% of carbon fiber, 0 - 2.54 wt.% of aluminum powder, and 5 - 50 wt.% of 304L stainless steel powder; all raw material powders are elemental powders with a purity of 99%; except that the carbon fiber has a length of 3 mm and a diameter of 7 nm, the other raw material powder particles are less than 45 μm.

[0028] The preparation method of the above novel metal-ceramic matrix composite is as follows:

[0029] (1) Several of titanium powder, silicon powder, graphite powder, carbon fiber, aluminum powder, and 304L stainless steel powder are ball-milled in a ball mill. The mass ratio of balls to materials is 2:1. The grinding balls are three types of hard alloy balls with different sizes of large, medium, and small (diameters are 6 mm, 4 mm, and 1 mm respectively), and the corresponding mass ratio of large, medium, and small balls is 1:3:6. The set rotation speed is 300 r / min, running alternately, stopping for 20 minutes every 1 hour, and the cumulative ball-milling time is 3 hours. After ball-milling, the raw material powder and the grinding balls are separated in a glove box to obtain a new metal-ceramic matrix composite powder.

[0030] (2) The raw material powder after ball-milling is filled into a hard alloy mold, pre-pressed and formed under a pressure of 100 MPa, and then put into a graphite mold for spark plasma sintering. The sintering pressure is 20 - 50 MPa, the sintering temperature is 1200 - 1600 °C, rising from room temperature to the target temperature at a rate of 50 - 90 °C / min, and keeping warm for 1 - 60 minutes after reaching the target temperature to obtain a sintered body of the new metal-ceramic matrix composite.

[0031] (3) The surface of the sintered body prepared in step (2) is polished to remove the residual graphite on the surface of the sample sintered body and the burrs generated at the edges during the sintering process, thereby obtaining the new metal-ceramic matrix composite.

[0032] The present invention relates to the preparation of a new metal-ceramic matrix composite. The prepared new metal-ceramic matrix composite has excellent mechanical properties and good friction properties at room temperature and high temperature, so as to ensure that the new metal-ceramic matrix composite meets the requirements of practical applications. The present invention has high practical application value.

[0033] Example 1

[0034] By mass percentage, 67.12 wt.% of titanium powder, 12.88 wt.% of silicon powder, 10 wt.% of graphite powder, 0 wt.% of carbon fiber, 0 wt.% of aluminum powder, and 10 wt.% of 304L stainless steel powder are put into a WC hard alloy tank. The purity of all raw material powders is 99%, the mesh number is 200 mesh, the ball-milling medium is WC hard alloy balls. After repeated gas washing (argon gas) in the glove box transition chamber, it is put into the operation cavity, the sealing cover is covered, and it is taken out in an argon environment in the tank and put into the ball mill. The ball-to-material ratio is 10:1, the ball-milling rotation speed is 200 r / min, running alternately forward and backward, running forward for 1 hour and stopping for 30 minutes, then running backward for 1 hour, repeating in cycles. After ball-milling for 3 hours, all the powder materials are taken out.

[0035] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 300 MPa using a hydraulic press, the obtained preform is placed into a spark plasma system for sintering experiments. The experiment is carried out at a sintering temperature of 1200 °C under 20 MPa, with a heating rate of 80 °C / min, holding for 10 min at 1200 °C, then unloading the pressure and slowly cooling to room temperature to obtain a new metal-ceramic matrix composite. The XRD pattern of the new metal-ceramic matrix composite prepared in this example is as shown in Figure 1 shown. The fracture FESEM image of the new metal-ceramic matrix composite prepared in this example is as shown in Figure 2 shown. The room-temperature friction surface FESEM image of the new metal-ceramic matrix composite prepared in this example is as shown in Figure 3 shown.

[0036] After grinding and polishing the prepared new metal-ceramic matrix composite, it is subjected to microstructure and property tests using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0037]

[0038] Example 2

[0039] By mass percentage, 67.12 wt.%, 12.88 wt.%, 10 wt.%, 0 wt.%, 0 wt.%, 10 wt.% of titanium powder, silicon powder, graphite powder, carbon fiber, aluminum powder, 304L stainless steel powder are put into a WC cemented carbide tank. The purity of all raw material powders is 99%, the mesh number is 200, the ball-milling medium is WC cemented carbide balls. After repeated gas washing (argon) in the glove box transfer chamber, it is put into the operation cavity, the sealing cover is covered, and it is taken out in an argon environment in the tank and put into a ball mill. The ball-to-material ratio is 10:1, the ball-milling speed is 200 r / min, running alternately forward and backward, running forward for 1 h and stopping for 30 min, then running backward for 1 h, repeating in cycles. After ball-milling for 3 h, all the powder materials are taken out.

[0040] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 300 MPa using a hydraulic press, the obtained preform is placed into a spark plasma system for sintering experiments. The experiment is carried out at a sintering temperature of 1400 °C under 20 MPa, with a heating rate of 80 °C / min, holding for 10 min at 1400 °C, then unloading the pressure and slowly cooling to room temperature to obtain a new metal-ceramic matrix composite.

[0041] After grinding and polishing the prepared new metal-ceramic matrix composite, it is subjected to microstructure and property tests using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0042]

[0043] Example 3

[0044] By mass percentage, 67.12 wt.% of titanium powder, 12.88 wt.% of silicon powder, 10 wt.% of graphite powder, 0 wt.% of carbon fiber, 0 wt.% of aluminum powder, and 10 wt.% of 304L stainless steel powder are put into a WC hard alloy tank. The purity of all raw material powders is 99%, the mesh number is 200 mesh, the ball milling medium is WC hard alloy balls. After repeated gas washing (argon) in the glove box transition chamber, it is put into the operation cavity, the sealing cover is covered, and it is taken out in an argon environment in the tank and put into a ball mill. The ball-to-material ratio is 10:1, the ball milling speed is 200 r / min, and it runs alternately forward and backward. It runs forward for 1 h and stops for 30 min, then runs backward for 1 h, and repeats in cycles. After ball milling for 3 h, all the powder materials are taken out.

[0045] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 300 MPa with a hydraulic press, the obtained preform is put into a spark plasma system for sintering experiments. The experiment is carried out at a sintering temperature of 1600 °C under 20 MPa, the heating rate is 80 °C / min, it is kept at 1600 °C for 10 min, then the pressure is unloaded and slowly cooled to room temperature to obtain a new metal-ceramic matrix composite material.

[0046] After grinding and polishing the obtained new metal-ceramic matrix composite material, it is tested for its microstructure and properties using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0047]

[0048] Example 4

[0049] By mass percentage, 35.74 wt.% of titanium powder, 6.97 wt.% of silicon powder, 0 wt.% of graphite powder, 5.65 wt.% of carbon fiber, 1.64 wt.% of aluminum powder, and 50 wt.% of 304L stainless steel powder are put into a WC hard alloy tank. The purity of all raw material powders is 99%, the ball-to-material ratio is 2:1, the ball milling medium is WC hard alloy balls. After repeated gas washing (argon) in the glove box transition chamber, it is put into the operation cavity, the sealing cover is covered, and it is taken out in an argon environment in the tank and put into a ball mill. The ball milling speed is 200 r / min, and it runs alternately forward and backward. It runs forward for 1 h and stops for 30 min, then runs backward for 1 h, and repeats in cycles. After ball milling for 10 h, all the powder materials are taken out.

[0050] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 50 MPa using a hydraulic press, the obtained preform is placed into a spark plasma system for sintering experiments. The experiments are carried out at a sintering temperature of 1200 °C under 50 MPa, with a heating rate of 90 °C / min, holding for 30 min at 1200 °C, then unloading the pressure and slowly cooling to room temperature to obtain a new metal-ceramic matrix composite material.

[0051] After grinding and polishing the obtained new metal-ceramic matrix composite material, it is subjected to microstructure and property tests using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0052]

[0053] Example 5

[0054] By mass percentage, 35.74 wt.% titanium powder, 6.97 wt.% silicon powder, 0 wt.% graphite powder, 5.65 wt.% carbon fiber, 1.64 wt.% aluminum powder, and 50 wt.% 304L stainless steel powder are put into a WC cemented carbide tank. The purity of all raw material powders is 99%. The ball-to-material ratio is 2:1, and the ball-milling medium is WC cemented carbide balls. After repeated gas washing (argon) in the glove box transition chamber, it is placed into the operation cavity, the sealing cover is covered, and it is taken out in an argon environment in the tank and put into a ball mill. The ball-milling speed is 200 r / min, running alternately forward and backward, running forward for 1 h and stopping for 30 min, then running backward for 1 h, and repeating in cycles. After ball-milling for 10 h, all the powder materials are taken out.

[0055] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 50 MPa using a hydraulic press, the obtained preform is placed into a spark plasma system for sintering experiments. The experiments are carried out at a sintering temperature of 1400 °C under 50 MPa, with a heating rate of 90 °C / min, holding for 30 min at 1400 °C, then unloading the pressure and slowly cooling to room temperature to obtain a new metal-ceramic matrix composite material.

[0056] After grinding and polishing the obtained new metal-ceramic matrix composite material, it is subjected to microstructure and property tests using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0057]

[0058] Example 6

[0059] By mass percentage, 35.74 wt.% of titanium powder, 6.97 wt.% of silicon powder, 0 wt.% of graphite powder, 5.65 wt.% of carbon fiber, 1.64 wt.% of aluminum powder, and 50 wt.% of 304L stainless steel powder are placed into a WC cemented carbide can. The purity of all raw material powders is 99%. The ball-to-material ratio is 2:1, and the ball-milling medium is WC cemented carbide balls. After repeated gas washing (argon gas) in the glove box transition chamber, it is placed into the operation cavity, the sealing cover is covered, and it is taken out under an argon gas environment in the can and placed into a ball mill. The ball-milling speed is 200 r / min, with forward and reverse rotations alternating. It runs forward for 1 h and stops for 30 min, then runs in reverse for 1 h, repeating in cycles. After ball-milling for 10 h, all the powder materials are taken out.

[0060] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 50 MPa using a hydraulic press, the obtained preform is placed into a spark plasma system for sintering experiments. The experiment uses a sintering temperature of 1600 °C at 50 MPa, a heating rate of 90 °C / min, holds at 1600 °C for 30 min, then unloads the pressure and slowly cools down to room temperature to obtain a new metal-ceramic matrix composite material.

[0061] After grinding and polishing the obtained new metal-ceramic matrix composite material, it is subjected to microstructure and property tests using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0062]

[0063] Example 7

[0064] By mass percentage, 61.10 wt.% of titanium powder, 11.92 wt.% of silicon powder, 5 wt.% of graphite powder, 10.18 wt.% of carbon fiber, 2.30 wt.% of aluminum powder, and 9.5 wt.% of 304L stainless steel powder are placed into a WC cemented carbide can. The purity of all raw material powders is 99%. The ball-to-material ratio is 2:1, and the ball-milling medium is WC cemented carbide balls. After repeated gas washing (argon gas) in the glove box transition chamber, it is placed into the operation cavity, the sealing cover is covered, and it is taken out under an argon gas environment in the can and placed into a ball mill. The ball-milling speed is 400 r / min, with forward and reverse rotations alternating. It runs forward for 1 h and stops for 30 min, then runs in reverse for 1 h, repeating in cycles. After ball-milling for 5 h, all the powder materials are taken out.

[0065] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 100 MPa using a hydraulic press, the obtained preform is placed into a spark plasma system for sintering experiments. The experiment is carried out at a sintering temperature of 1200 °C under 40 MPa, with a heating rate of 60 °C / min, holding for 30 min at 1200 °C, then unloading the pressure and slowly cooling to room temperature to obtain a novel metal-ceramic matrix composite. The XRD pattern of the novel metal-ceramic matrix composite prepared in this example is as shown in Figure 4 shown. The fracture FESEM image of the novel metal-ceramic matrix composite prepared in this example is as shown in Figure 5 shown. The FESEM image of the room-temperature friction surface of the novel metal-ceramic matrix composite prepared in this example is as shown in Figure 6 shown.

[0066] After grinding and polishing the prepared novel metal-ceramic matrix composite, it is subjected to microstructure and property tests using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0067]

[0068] Example 8

[0069] By mass percentage, 61.10 wt.% titanium powder, 11.92 wt.% silicon powder, 5 wt.% graphite powder, 10.18 wt.% carbon fiber, 2.30 wt.% aluminum powder, and 9.5 wt.% 304L stainless steel powder are put into a WC cemented carbide tank. The purity of all raw material powders is 99%. The ball-to-material ratio is 2:1, and the ball-milling medium is WC cemented carbide balls. After repeated gas washing (argon) in the glove box transfer chamber, it is placed into the operation cavity, the sealing cover is covered, and it is taken out under an argon atmosphere in the tank and put into a ball mill. The ball-milling speed is 400 r / min, running alternately forward and backward, running forward for 1 h and stopping for 30 min, then running backward for 1 h, and repeating in cycles. After ball-milling for 5 h, all the powder is taken out.

[0070] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 100 MPa using a hydraulic press, the obtained preform is placed into a spark plasma system for sintering experiments. The experiment is carried out at a sintering temperature of 1400 °C under 40 MPa, with a heating rate of 60 °C / min, holding for 30 min at 1400 °C, then unloading the pressure and slowly cooling to room temperature to obtain a novel metal-ceramic matrix composite.

[0071] After grinding and polishing the prepared novel metal-ceramic matrix composite, it is subjected to microstructure and property tests using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0072]

[0073]

[0074] Example 9

[0075] By mass percentage, 61.10 wt.% of titanium powder, 11.92 wt.% of silicon powder, 5 wt.% of graphite powder, 10.18 wt.% of carbon fiber, 2.30 wt.% of aluminum powder, and 9.5 wt.% of 304L stainless steel powder are put into a WC cemented carbide tank. The purity of all raw material powders is 99%. The ball-to-material ratio is 2:1, and the ball-milling medium is WC cemented carbide balls. After repeated gas washing (argon gas) in the glove box transition chamber, it is put into the operation cavity, the sealing cover is covered, and it is taken out under an argon gas environment in the tank and put into a ball mill. The ball-milling speed is 400 r / min, running alternately forward and backward, running forward for 1 h and stopping for 30 min, then running backward for 1 h, repeating in cycles. After ball-milling for 5 h, all the powder materials are taken out.

[0076] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 100 MPa by a hydraulic press, the obtained preform is put into a spark plasma system for sintering experiments. The experiment uses a sintering temperature of 1600 °C at 40 MPa, a heating rate of 60 °C / min, holding at 1600 °C for 30 min, then unloading the pressure and slowly cooling to room temperature to obtain a new metal-ceramic matrix composite material.

[0077] After grinding and polishing the obtained new metal-ceramic matrix composite material, it is tested for its microstructure and properties using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0078]

[0079] Example 10

[0080] By mass percentage, 61.10 wt.% of titanium powder, 11.92 wt.% of silicon powder, 5 wt.% of graphite powder, 10.18 wt.% of carbon fiber, 2.30 wt.% of aluminum powder, and 9.5 wt.% of 304L stainless steel powder are put into a WC cemented carbide tank. The purity of all raw material powders is 99%. The ball-to-material ratio is 2:1, and the ball-milling medium is WC cemented carbide balls. After repeated gas washing (argon gas) in the glove box transition chamber, it is put into the operation cavity, the sealing cover is covered, and it is taken out under an argon gas environment in the tank and put into a ball mill. The ball-milling speed is 400 r / min, running alternately forward and backward, running forward for 1 h and stopping for 30 min, then running backward for 1 h, repeating in cycles. After ball-milling for 5 h, all the powder materials are taken out.

[0081] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 100 MPa using a hydraulic press, the obtained preform is placed into a spark plasma system for sintering experiments. The experiment is carried out at a sintering temperature of 1600 °C under 40 MPa, with a heating rate of 60 °C / min, holding for 10 min at 1600 °C, then unloading the pressure and slowly cooling to room temperature to obtain a new metal-ceramic matrix composite material.

[0082] After grinding and polishing the obtained new metal-ceramic matrix composite material, it is subjected to microstructure and property tests using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0083]

[0084] Example 11

[0085] By mass percentage, 61.10 wt.% titanium powder, 11.92 wt.% silicon powder, 5 wt.% graphite powder, 10.18 wt.% carbon fiber, 2.30 wt.% aluminum powder, and 9.5 wt.% 304L stainless steel powder are placed into a WC hard alloy can. The purity of all raw material powders is 99%. The ball-to-material ratio is 2:1, and the ball-milling medium is WC hard alloy balls. After repeated gas washing (argon) in the glove box transfer chamber, it is placed into the operation cavity, the sealing cover is covered, and it is taken out under an argon environment in the can and placed into a ball mill. The ball-milling speed is 400 r / min, running alternately forward and backward, running forward for 1 h and stopping for 30 min, then running backward for 1 h, and repeating in cycles. After ball-milling for 5 h, all the powder materials are taken out.

[0086] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming under a pressure of 100 MPa using a hydraulic press, the obtained preform is placed into a spark plasma system for sintering experiments. The experiment is carried out at a sintering temperature of 1600 °C under 40 MPa, with a heating rate of 60 °C / min, holding for 1 min at 1600 °C, then unloading the pressure and slowly cooling to room temperature to obtain a new metal-ceramic matrix composite material.

[0087] After grinding and polishing the obtained new metal-ceramic matrix composite material, it is subjected to microstructure and property tests using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0088]

[0089] Example 12

[0090] By mass percentage, 67.12 wt.% of titanium powder, 12.88 wt.% of silicon powder, 10 wt.% of graphite powder, 0 wt.% of carbon fiber, 0 wt.% of aluminum powder, and 10 wt.% of 304L stainless steel powder are put into a WC cemented carbide tank. The purity of all raw material powders is 99%, the mesh number is 200 mesh, the ball milling medium is WC cemented carbide balls. After repeated gas washing (argon) in the glove box transition chamber, it is put into the operation cavity, the sealing cover is covered, and it is taken out under the argon environment in the tank and put into the ball mill. The ball-to-material ratio is 10:1, the ball milling speed is 200 r / min, and it runs alternately forward and backward. It runs forward for 1 h and stops for 30 min, then runs backward for 1 h, and repeats in cycles. After ball milling for 3 h, all the powder materials are taken out.

[0091] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper, pre-pressed into shape by a hydraulic press at a pressure of 300 MPa, and then the obtained preform is put into a spark plasma system for sintering experiments. The experiment uses a sintering temperature of 1600 °C at 20 MPa, a heating rate of 50 °C / min, holds for 10 min at 1600 °C, then unloads the pressure and slowly cools down to room temperature to obtain a new metal-ceramic matrix composite material.

[0092] The obtained new metal-ceramic matrix composite material is polished and then detected for its microstructure and properties using the instruments for conventional detection means. The obtained technical parameters are as follows:

[0093]

[0094] Example 13

[0095] By mass percentage, 67.12 wt.% of titanium powder, 12.88 wt.% of silicon powder, 10 wt.% of graphite powder, 0 wt.% of carbon fiber, 0 wt.% of aluminum powder, and 10 wt.% of 304L stainless steel powder are put into a WC cemented carbide tank. The purity of all raw material powders is 99%, the mesh number is 200 mesh, the ball milling medium is WC cemented carbide balls. After repeated gas washing (argon) in the glove box transition chamber, it is put into the operation cavity, the sealing cover is covered, and it is taken out under the argon environment in the tank and put into the ball mill. The ball-to-material ratio is 10:1, the ball milling speed is 200 r / min, and it runs alternately forward and backward. It runs forward for 1 h and stops for 30 min, then runs backward for 1 h, and repeats in cycles. After ball milling for 3 h, all the powder materials are taken out.

[0096] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper, pre-pressed into shape by a hydraulic press at a pressure of 300 MPa, and then the obtained preform is put into a spark plasma system for sintering experiments. The experiment uses a sintering temperature of 1600 °C at 20 MPa, a heating rate of 90 °C / min, holds for 10 min at 1600 °C, then unloads the pressure and slowly cools down to room temperature to obtain a new metal-ceramic matrix composite material.

[0097] After polishing the prepared new cermet matrix composite material, use the instruments used in conventional testing methods to detect its microstructure and properties. The obtained technical parameters are as follows:

[0098]

[0099] Example 14

[0100] By mass percentage, 35.74 wt.% titanium powder, 6.97 wt.% silicon powder, 0 wt.% graphite powder, 5.65 wt.% carbon fiber, 1.64 wt.% aluminum powder, and 50 wt.% 304L stainless steel powder are put into a WC cemented carbide tank. The purity of all raw material powders is 99%. The ball-to-material ratio is 2:1, and the ball-milling medium is WC cemented carbide balls. After repeatedly purging with argon in the glove box transfer chamber, it is put into the operation cavity, the sealing cover is covered, and it is taken out and put into the ball mill under an argon environment in the tank. The ball-milling speed is 200 r / min, with forward and reverse rotation alternating. It runs forward for 1 h and stops for 30 min, then runs in reverse for 1 h, and so on. After ball-milling for 10 h, all the powder is taken out.

[0101] Fill the ball-milled raw material powder into a graphite mold pre-lined with graphite gasket paper, pre-press it into shape with a hydraulic press at a pressure of 50 MPa, and then put the obtained preform into a spark plasma system for sintering experiments. The experiment is carried out at a sintering temperature of 1400 °C under 30 MPa, with a heating rate of 90 °C / min, holding for 30 min at 1400 °C, then unloading the pressure and slowly cooling to room temperature to obtain the new cermet matrix composite material.

[0102] After polishing the prepared new cermet matrix composite material, use the instruments used in conventional testing methods to detect its microstructure and properties. The obtained technical parameters are as follows:

[0103]

[0104] Example 15

[0105] By mass percentage, 35.74 wt.% titanium powder, 6.97 wt.% silicon powder, 0 wt.% graphite powder, 5.65 wt.% carbon fiber, 1.64 wt.% aluminum powder, and 50 wt.% 304L stainless steel powder are put into a WC cemented carbide tank. The purity of all raw material powders is 99%. The ball-to-material ratio is 2:1, and the ball-milling medium is WC cemented carbide balls. After repeatedly purging with argon in the glove box transfer chamber, it is put into the operation cavity, the sealing cover is covered, and it is taken out and put into the ball mill under an argon environment in the tank. The ball-milling speed is 200 r / min, with forward and reverse rotation alternating. It runs forward for 1 h and stops for 30 min, then runs in reverse for 1 h, and so on. After ball-milling for 10 h, all the powder is taken out.

[0106] The ball-milled raw material powder is filled into a graphite mold pre-lined with graphite gasket paper. After pre-pressing and forming at a pressure of 50 MPa using a hydraulic press, the obtained preform is placed in a spark plasma system for sintering experiments. The experiments are carried out at a sintering temperature of 1400 °C under 20 MPa, with a heating rate of 90 °C / min, holding for 30 min at 1400 °C, and then unloading the pressure and slowly cooling to room temperature to obtain the new metal-ceramic matrix composite material.

[0107] The obtained new metal-ceramic matrix composite material is polished and then tested for its microstructure and properties using the instruments for conventional testing methods. The obtained technical parameters are as follows:

[0108]

[0109] From Examples 1-3, it can be seen that when the raw materials are Ti, Si, C, and 304L stainless steel, with the increase of the sintering temperature, the bulk density, relative density, hardness, and toughness of the new metal-ceramic matrix composite material gradually increase, while the friction coefficients and wear rates at room temperature and 500 °C gradually decrease.

[0110] From Examples 4-6, it can be seen that when the raw materials are Ti, Si, Cf, Al, and 304L stainless steel, with the increase of the sintering temperature, the bulk density, relative density, hardness, and toughness of the new metal-ceramic matrix composite material gradually increase, while the friction coefficients and wear rates at room temperature and 500 °C gradually decrease.

[0111] From Examples 7-9, it can be seen that when the raw materials are Ti, Si, Cf, C, Al, and 304L stainless steel, with the increase of the sintering temperature, the bulk density, relative density, hardness, toughness, friction coefficients at room temperature and 500 °C, and wear rates of the new metal-ceramic matrix composite material gradually increase.

[0112] From Examples 9-11, it can be seen that with the increase of the holding time, the bulk density, relative density, hardness, toughness, friction coefficients at room temperature and 500 °C, and wear rates of the new metal-ceramic matrix composite material all gradually decrease.

[0113] From Examples 3, 12, and 13, it can be seen that with the increase of the heating rate, the bulk density, relative density, hardness, and toughness of the new metal-ceramic matrix composite material gradually increase, while the friction coefficients and wear rates at room temperature and 500 °C gradually decrease.

[0114] From Examples 5, 14, and 15, it can be seen that with the increase of the heating rate, the bulk density, relative density, hardness, and toughness of the new metal-ceramic matrix composite material gradually increase, while the friction coefficients and wear rates at room temperature and 500 °C gradually decrease.

[0115] The novel cermet matrix composite material prepared by the present invention has great advantages in mechanical and friction properties compared with other novel cermet matrix composite materials, and has great practical application value.

[0116] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some or all of the technical features. These modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A new cermet-based composite material, characterized in that, The composite material is composed of materials with the following weight ratios: titanium powder 35.74 - 67.12 wt.%, silicon powder 6.97 - 12.88 wt.%, graphite powder 0 - 10 wt.%, carbon fiber 0 - 10.72 wt.%, aluminum powder 0 - 2.54 wt.%, 304L stainless steel powder 5 - 50 wt.%. The titanium powder, silicon powder, graphite powder, aluminum powder, and 304L stainless steel powder are elemental powders; the purity of the titanium powder, silicon powder, graphite powder, aluminum powder, and 304L stainless steel powder is 99%; the particle diameters of the titanium powder, silicon powder, graphite powder, aluminum powder, and 304L stainless steel powder are less than 45 μm; the length of the carbon fiber is 3 mm and the diameter is 7 nm.

2. A method for preparing a novel cermet matrix composite material, which is used to prepare the novel cermet matrix composite material described in claim 1, and is characterized in that, It includes the following steps: S1. Ball-mill several of the titanium powder, silicon powder, graphite powder, carbon fiber, aluminum powder, and 304L stainless steel powder in a ball mill. The mass ratio of balls to materials ranges from 2:1 to 10:

1. After ball-milling, separate the raw material powder from the grinding balls in a glove box to obtain the novel metal-ceramic matrix composite material powder. S2. Fill the novel metal-ceramic matrix composite material powder obtained in S1 into a cemented carbide mold, pre-press it under a pressure of 50 - 300 MPa, then load it into a graphite mold for spark plasma sintering. The sintering pressure is 20 - 50 MPa, the sintering temperature is 1200 - 1600 °C, raise the temperature from room temperature to the target sintering temperature at a rate of 50 - 90 °C / min, and keep it at the target sintering temperature for 1 - 60 min to obtain the sintered body of the novel metal-ceramic matrix composite material. S3. Grind and polish the surface of the sintered body obtained in S2 to remove the residual graphite on the surface of the sintered body and the burrs generated at the edges during the sintering process, thereby obtaining the novel metal-ceramic matrix composite material.

3. The preparation method of the novel cermet matrix composite material according to claim 2, characterized in that, In S1, the grinding balls are three kinds of cemented carbide balls with different sizes: the large-sized cemented carbide ball has a diameter of 6 mm, the medium-sized cemented carbide ball has a diameter of 4 mm, and the small-sized cemented carbide ball has a diameter of 1 mm. The mass ratio of the three kinds of cemented carbide balls with different sizes is 1:3:

6.

4. The preparation method of the novel cermet matrix composite material according to claim 2, wherein, In S1, set the rotation speed range to 200 - 400 r / min, run in forward and reverse alternately, stop for 20 - 30 min every 1 h, and the cumulative ball-milling time range is 3 - 10 h.

Citation Information

Patent Citations

  • Aluminum oxide enhanced titanium-silicon-aluminum-carbon base ceramics composite material and preparing method thereof

    CN101033135A